CN112758924B - Graphene material composite biomass activated carbon and preparation method thereof - Google Patents

Graphene material composite biomass activated carbon and preparation method thereof Download PDF

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CN112758924B
CN112758924B CN202110286832.4A CN202110286832A CN112758924B CN 112758924 B CN112758924 B CN 112758924B CN 202110286832 A CN202110286832 A CN 202110286832A CN 112758924 B CN112758924 B CN 112758924B
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activated carbon
graphene
composite biomass
biomass activated
culture medium
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CN112758924A (en
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郑群
毛婷
王沛雅
方彦昊
季彬
王治业
杨晖
祝英
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Institute of Biology of Gansu Academy of Sciences
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Institute of Biology of Gansu Academy of Sciences
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/336—Preparation characterised by gaseous activating agents

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Abstract

The invention discloses a method for forming a hypha complex adsorbing graphene materials in the growth process of fungi by introducing the graphene materials, and then forming an activated carbon material compounded by the graphene materials through carbonization treatment, and a graphene material composite biomass activated carbon prepared by the method. The method provided by the invention has the advantages of simple process, strong controllability and low cost, can provide a new thought and a production way for developing high-performance, low-cost and high-efficiency biomass activated carbon and composite biomass activated carbon materials, and has the potential of large-scale industrial production.

Description

Graphene material composite biomass activated carbon and preparation method thereof
Technical Field
The invention relates to the field of new material preparation, in particular to graphene material composite biomass activated carbon and a preparation method thereof.
Background
The activated carbon has the advantages of rich pores, high specific surface area, good adsorption performance and stability and the like, and is widely applied to the fields of catalytic degradation, sewage treatment, air purification, energy storage devices and the like. In addition, the method has great significance in the aspects of food, chemical industry, medicine, environmental protection and the like. The activated carbon has the characteristics of acid resistance, alkali resistance, heat resistance, convenient regeneration and the like, so that the activated carbon plays more and more important roles in protecting the environment and improving the quality of life of human beings. In recent years, research on the preparation of activated carbon by using biomass materials as precursors has attracted great attention in the above-mentioned fields. The biomass material refers to any renewable or recyclable organic matter, including plant, animal, microorganism and other organic matters, and has the characteristics of low price, rich sources, environmental friendliness and the like. The biomass material has low ash content and moderate hardness, and is a high-quality resource for preparing the active carbon. At present, biomass activated carbon products are mainly prepared from agricultural wastes such as wood chips, charcoal, coconut shells, walnut shells, apricot shells and the like as raw materials. These biomass activated carbons generally have the disadvantages of difficult impurity removal, low adsorption capacity, optimized performance, etc. and have prompted the search for higher performance activated carbons.
The microorganism has the advantages of various types, various shapes, more abundant micro-morphology and the like, and can become an ideal biomass active carbon precursor material. It not only exists widely in nature, but also can be cultivated in a large scale by means of artificial cultivation. The required target activated carbon material can be prepared by selecting the micro-morphology of the microbial precursor, and the biomass activated carbon with different properties can be prepared by introducing other additives to form a composite biomass precursor in the microbial growth process. Pythium oligandrum (A), (B), (C), (B), (C)Pythium oligandrum) Is an environment-friendly and harmless beneficial fungus for people and livestock in the nature, and also has a specific morphological structure. For the modification of activated carbon, graphene-based materials are an ideal choice due to a variety of excellent properties. For example, graphene has a wide application in many fields due to its excellent electrical properties, optical properties, biocompatibility, and other properties, and similar materials include graphene oxide and MoS2、WS2MXene, etc. However, how to effectively compound the material with biomass carbon to improve the performance of the material is not reported.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a graphene material composite biomass activated carbon and a preparation method thereof.
The invention aims to provide a preparation method of graphene material composite biomass activated carbon, which specifically comprises the following steps:
(1) adding the graphene material into a fungus culture medium, and uniformly stirring, wherein the addition amount is 5-1000 mg/L;
(2) inoculating fungus into the above culture medium, standing at room temperature or standing at 28 deg.CoC shaking culture in constant temperature shaking table at 150r/min untilA large amount of flocculent hypha complexes grow, and the culture medium is clear and bright;
(3) taking out the mycelium complex, and washing off the culture medium attached to the mycelium complex by using deionized water;
(4) placing the washed mycelium complex in a calcining furnace 600oAnd C, carbonizing for 1 hour, and continuously introducing argon for protection to obtain the graphene material composite biomass activated carbon material.
Preferably, the composite biomass activated carbon material obtained in the step (4) can be prepared at 200oAnd C, introducing water vapor for 2-30min to obtain the water activated graphene material composite biomass activated carbon.
Preferably, the graphene-based material in step (1) is graphene, graphene oxide, Maxene, MoS2、WS2Or other relevant material.
Preferably, the fungus culture medium in the step (1) is PDA or V8 liquid culture medium.
Preferably, the fungus used in step (2) is Pythium oligandrum, or other fungus such as Trichoderma reesei.
Preferably, the washed mycelial complex obtained in step (3) is lyophilized and then subjected to step (4).
The second purpose of the invention is to provide the graphene material composite biomass activated carbon prepared by the method.
The invention provides a method for forming high-quality graphene material composite biomass activated carbon by using microorganisms as precursors, introducing functional materials in the growth process of the microorganisms to form biomass precursors and then carrying out carbonization treatment. The graphene material is introduced into the growth process of fungi to form a compound adsorbed with the graphene material, the original morphology of the polytetramer can be kept by performing a freeze-drying treatment process on the hypha compound, and then the graphene material composite activated carbon is formed through carbonization treatment.
The biomass active carbon with excellent performance can be obtained by adopting the method, and the characteristics of the composite active carbon can be effectively improved by adding the graphene material, so that the composite active carbon has better performance. The performance of the composite biomass activated carbon can be effectively adjusted by controlling the addition of the graphene material. The preparation process is simple, the requirement on production equipment is low, and the preparation method is suitable for large-scale production. The successful application of the invention can not only solve the preparation problem of the high-quality biomass activated carbon, but also provide a new method for preparing the functional material composite activated carbon, and the prepared composite biomass carbon can be used in the fields of catalysis, energy storage, adsorption, air purification and the like, and can bring huge economic, environmental protection and social benefits.
Drawings
Fig. 1 is a microscopic topography of a low concentration graphene oxide composite biomass activated carbon prepared in example 1.
Fig. 2 is a microscopic topography of the medium concentration graphene oxide composite biomass activated carbon prepared in example 2.
Fig. 3 is a carbon micro-topography of the high concentration graphene oxide composite biomass activated carbon prepared in example 3.
Fig. 4 a microscopic morphology of the high concentration graphene composite biomass activated carbon prepared in example 4.
FIG. 5 is a single or few layer MoS prepared in example 52A microscopic morphology of the composite biomass activated carbon.
Figure 6 is a raman spectrum of a medium concentration graphene oxide composite biomass activated carbon prepared in example 2.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope defined by the present application.
In the following examples, the Pythium oligandrum strain was deposited at the institute of biological research, national academy of sciences of Gansu province, and other reagents were commercially available.
The media formulations used in the following examples were as follows:
PDA liquid culture medium: weighing 200g of potato, cleaning, peeling, cutting into pieces, adding 1000ml of water, boiling for half an hour, filtering with gauze, adding 20g of glucose, and sterilizing with high-pressure steam at 121 deg.C for 20 min;
v8 liquid medium: 200 mL of V8 juice, CaCO33 g, adding distilled water to 1000mL, and autoclaving at 121 ℃ for 20 min.
Example 1
And (3) selecting pythium oligandrum strains and a PDA liquid culture medium to adsorb low-concentration graphene oxide, and preparing the low-concentration graphene oxide composite biomass activated carbon.
The PDA culture medium is subpackaged into 100mL conical flasks, each flask is 40mL, and pythium oligandrum strain is inoculated. Adding graphene oxide according to the concentration of 5mg/L, shaking up, and adding the mixture at 28 DEGoC, shake culturing for 5-7 days at 150r/min in a constant temperature shaking table until a large amount of flocculent hypha complexes grow, and the culture medium is clear and bright. Taking out the mycelium complex, and washing off the culture medium attached to the mycelium complex by using deionized water; washing, freeze-drying in a freeze dryer to maintain its original shape, and calcining in a calcining furnace 600oAnd C, carbonizing for 1 hour, and continuously introducing argon for protection during the carbonization, so that the low-concentration graphene oxide composite biomass activated carbon material can be obtained. Finally, the composite biomass activated carbon material is 200oAnd C, introducing water vapor for 2-30 minutes under the condition to obtain the water-activated low-concentration graphene oxide composite biomass activated carbon.
Example 2
And (3) selecting pythium oligandrum strains and a V8 liquid culture medium to adsorb medium-concentration graphene oxide, and preparing the medium-concentration graphene oxide composite biomass activated carbon.
The V8 liquid culture medium is subpackaged into 100mL conical flasks, and each flask is filled with 40mL, and the pythium oligandrum strain is inoculated. Adding graphene oxide according to the concentration of 100mg/L, shaking up, standing at room temperature and culturing until a large amount of flocculent hypha complexes grow out, wherein the culture medium is clear and bright. Taking out the mycelium complex, and washing off the culture medium attached to the mycelium complex by using deionized water; after being washed clean, the mixture is placed in a calcining furnace 600oAnd C, carbonizing for 1 hour, and continuously introducing argon for protection during the carbonization, so as to obtain the intermediate-concentration graphene oxide composite biomass activated carbon material. Finally, the composite biomass activated carbon material is 200oCondition CAnd introducing water vapor for 2-30 minutes to obtain the water-activated medium-concentration graphene oxide composite biomass activated carbon.
Fig. 2 is a raman spectrum of the prepared intermediate-concentration graphene oxide composite biomass activated carbon, and a G peak of the prepared biomass activated carbon material shown in fig. 2 is obviously higher than a D peak, which indicates that the graphitization degree is higher.
Example 3
And (3) carrying out high-concentration graphene oxide adsorption by using a pythium oligandrum strain and a PDA (potato dextrose agar) liquid culture medium to prepare the high-concentration graphene oxide composite biomass activated carbon.
The PDA culture medium is subpackaged into 100mL conical flasks, each flask is 40mL, and pythium oligandrum strain is inoculated. Adding graphene oxide according to the concentration of 1000mg/L, shaking up, and adding the mixture at 28 DEGoC, shake culturing for 5-7 days at 150r/min in a constant temperature shaking table until a large amount of flocculent hypha complexes grow, and the culture medium is clear and bright. Taking out the mycelium complex, and washing off the culture medium attached to the mycelium complex by using deionized water; washing, freeze-drying in a freeze dryer to maintain its original shape, and calcining in a calcining furnace 600oAnd C, carbonizing for 1 hour, and continuously introducing argon for protection during the carbonization, so as to obtain the high-concentration graphene oxide composite biomass activated carbon material.
Example 4
And (3) carrying out high-concentration graphene adsorption by using pythium oligandrum strains and a PDA (PDA) liquid culture medium to prepare the high-concentration graphene composite biomass activated carbon.
The PDA culture medium is subpackaged into 100mL conical flasks, each flask is 40mL, and pythium oligandrum strain is inoculated. Adding graphene according to the concentration of 1000mg/L, shaking up, and adding graphene at 28 DEGoC, shake culturing for 5-7 days at 150r/min in a constant temperature shaking table until a large amount of flocculent mycelium complexes grow, and the culture medium is clear and transparent. Taking out the mycelium complex, and washing off the culture medium attached to the mycelium complex by using deionized water; washing, freeze-drying in a freeze dryer to maintain its original shape, and calcining in a calcining furnace 600oAnd C, carbonizing for 1 hour, and continuously introducing argon for protection during the carbonization, so as to obtain the high-concentration graphene composite biomass activated carbon material. Finally, the composite biomass activated carbon material is 200oC stripAnd introducing water vapor for 2-30 minutes to obtain the water-activated high-concentration graphene composite biomass activated carbon.
Example 5
Selecting pythium oligandrum strain and PDA liquid culture medium to carry out monolayer or few-layer two-dimensional MoS2Adsorbing and preparing single-layer or few-layer two-dimensional MoS2Composite biomass activated carbon.
The PDA culture medium is subpackaged into 100mL conical flasks, each flask is 40mL, and pythium oligandrum strains are inoculated. Adding single-layer or few-layer two-dimensional MoS according to the concentration of 100mg/L2Shaking uniformly, and mixing at 28oC, shake culturing for 5-7 days at 150r/min in a constant temperature shaking table until a large amount of flocculent mycelium complexes grow, and the culture medium is clear and transparent. Taking out the mycelium complex, and washing off the culture medium attached to the mycelium complex by using deionized water; washing, freeze-drying in a freeze dryer to maintain its original shape, and calcining in a calcining furnace 600oCarbonizing C for 1 hour, and introducing argon gas for protection to obtain single-layer or few-layer two-dimensional MoS2Composite biomass activated carbon material. Finally, the composite biomass activated carbon material is 200oIntroducing water vapor for 2-30 minutes under the condition of C to obtain the water-activated single-layer or few-layer two-dimensional MoS2Composite biomass activated carbon.

Claims (4)

1. A preparation method of graphene material composite biomass activated carbon is characterized by comprising the following steps:
(1) mixing graphene, graphene oxide, Maxene and MoS2Or WS2Adding PDA or V8 liquid culture medium in an amount of 5-1000 mg/L;
(2) inoculating pythium oligandrum or trichoderma reesei, standing at room temperature or performing shake culture at 28 ℃ for 150r/min until flocculent hypha complexes grow out, and clarifying and brightening a culture medium;
(3) taking out the mycelium complex, and washing with deionized water;
(4) and (3) putting the washed hypha complex in a calcining furnace, carbonizing for 1h at 600 ℃, and continuously introducing argon for protection during the carbonization to obtain the graphene material composite biomass activated carbon.
2. The method for preparing graphene-based composite biomass activated carbon according to claim 1, wherein the graphene-based composite biomass activated carbon is subjected to steam at 200 ℃ for 2-30min to obtain the water-activated graphene-based composite biomass activated carbon.
3. The process for producing a graphene-based composite biomass activated carbon according to claim 1, wherein the washed mycelium complex obtained in step (3) is freeze-dried and then subjected to step (4).
4. A graphene-based composite biomass activated carbon, characterized in that it is prepared by any one of the methods of claims 1-3.
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CN114388786B (en) * 2021-12-21 2022-12-20 西安理工大学 Method for preparing carbon skeleton from wood hypha symbiotic material and application of sulfur-carrying energy storage
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